JP4540997B2 - Two-component casting epoxy resin composition and electrical / electronic component equipment - Google Patents
Two-component casting epoxy resin composition and electrical / electronic component equipment Download PDFInfo
- Publication number
- JP4540997B2 JP4540997B2 JP2004030449A JP2004030449A JP4540997B2 JP 4540997 B2 JP4540997 B2 JP 4540997B2 JP 2004030449 A JP2004030449 A JP 2004030449A JP 2004030449 A JP2004030449 A JP 2004030449A JP 4540997 B2 JP4540997 B2 JP 4540997B2
- Authority
- JP
- Japan
- Prior art keywords
- epoxy resin
- resin composition
- weight
- parts
- curing agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000003822 epoxy resin Substances 0.000 title claims description 57
- 229920000647 polyepoxide Polymers 0.000 title claims description 57
- 239000000203 mixture Substances 0.000 title claims description 43
- 238000005266 casting Methods 0.000 title claims description 34
- 239000003795 chemical substances by application Substances 0.000 claims description 91
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 41
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 26
- 239000000347 magnesium hydroxide Substances 0.000 claims description 25
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 25
- 229910019142 PO4 Inorganic materials 0.000 claims description 21
- 239000010452 phosphate Substances 0.000 claims description 21
- -1 phosphate ester Chemical class 0.000 claims description 19
- 239000000377 silicon dioxide Substances 0.000 claims description 19
- 150000008065 acid anhydrides Chemical class 0.000 claims description 18
- 150000001463 antimony compounds Chemical class 0.000 claims description 12
- 150000002366 halogen compounds Chemical class 0.000 claims description 11
- 239000012749 thinning agent Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 239000011342 resin composition Substances 0.000 claims description 4
- 229920000728 polyester Polymers 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims 1
- 150000008064 anhydrides Chemical class 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 239000000047 product Substances 0.000 description 16
- 239000002562 thickening agent Substances 0.000 description 12
- 239000011259 mixed solution Substances 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 7
- 238000000354 decomposition reaction Methods 0.000 description 7
- 239000003063 flame retardant Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 5
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000009477 glass transition Effects 0.000 description 3
- 239000011256 inorganic filler Substances 0.000 description 3
- 229910003475 inorganic filler Inorganic materials 0.000 description 3
- 239000002075 main ingredient Substances 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 2
- MUTGBJKUEZFXGO-OLQVQODUSA-N (3as,7ar)-3a,4,5,6,7,7a-hexahydro-2-benzofuran-1,3-dione Chemical compound C1CCC[C@@H]2C(=O)OC(=O)[C@@H]21 MUTGBJKUEZFXGO-OLQVQODUSA-N 0.000 description 1
- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 0.000 description 1
- RXFFQBYNCVPZGL-UHFFFAOYSA-N 1,2,3,4,5,5a,8,9-octahydropyrido[1,2-b]diazepine Chemical compound N1CCCCC2C=CCCN21 RXFFQBYNCVPZGL-UHFFFAOYSA-N 0.000 description 1
- ZOQVDXYAPXAFRW-UHFFFAOYSA-N 2,5-diethyl-1h-imidazole Chemical compound CCC1=CNC(CC)=N1 ZOQVDXYAPXAFRW-UHFFFAOYSA-N 0.000 description 1
- LXUMQTXVDSCWLS-UHFFFAOYSA-N 2-(2,5-diethyl-1H-imidazol-4-yl)propanenitrile Chemical compound C(#N)C(C)C1=C(N=C(N1)CC)CC LXUMQTXVDSCWLS-UHFFFAOYSA-N 0.000 description 1
- FUIQBJHUESBZNU-UHFFFAOYSA-N 2-[(dimethylazaniumyl)methyl]phenolate Chemical compound CN(C)CC1=CC=CC=C1O FUIQBJHUESBZNU-UHFFFAOYSA-N 0.000 description 1
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 description 1
- 229930185605 Bisphenol Natural products 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 125000004018 acid anhydride group Chemical group 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000001548 androgenic effect Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 229940058905 antimony compound for treatment of leishmaniasis and trypanosomiasis Drugs 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 229910002026 crystalline silica Inorganic materials 0.000 description 1
- 125000000113 cyclohexyl group Chemical class [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 1
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 1
- GPAYUJZHTULNBE-UHFFFAOYSA-N diphenylphosphine Chemical compound C=1C=CC=CC=1PC1=CC=CC=C1 GPAYUJZHTULNBE-UHFFFAOYSA-N 0.000 description 1
- 238000006735 epoxidation reaction Methods 0.000 description 1
- 150000002118 epoxides Chemical class 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- FIWHJQPAGLNURC-UHFFFAOYSA-N oxiran-2-ylmethyl 7,7-dimethyloctanoate Chemical compound CC(C)(C)CCCCCC(=O)OCC1CO1 FIWHJQPAGLNURC-UHFFFAOYSA-N 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- RXJKFRMDXUJTEX-UHFFFAOYSA-N triethylphosphine Chemical compound CCP(CC)CC RXJKFRMDXUJTEX-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
Description
本発明は２液性注形用エポキシ樹脂組成物およびそれを用いた電気・電子部品装置に係り、特にハロゲン化合物、アンチモン化合物を含まず、作業性に優れ、その硬化物の電気特性・難燃性および耐熱性に優れた２液性注形用エポキシ樹脂組成物およびそれを用いた電気・電子部品装置に関する。 The present invention relates to a two-part casting epoxy resin composition and an electric / electronic component device using the same, and particularly, does not contain a halogen compound or an antimony compound, has excellent workability, and has electrical properties and flame retardancy of the cured product. The present invention relates to a two-component casting epoxy resin composition excellent in heat resistance and heat resistance, and an electric / electronic component device using the same.
従来より、注形用エポキシ樹脂組成物は、電気機器用トランス類や電子部品封止などの絶縁処理に使用されている。このような注形用エポキシ樹脂組成物には、使用時における電気特性を含む諸特性の安定性および難燃性が要求されている。近年では、信頼性の向上と共に環境への配慮の点からハロゲン化合物やアンチモン化合物を含まない注形用エポキシ樹脂組成物が求められており、実用化されているものもある。また、近年では、電子部品に対する耐熱要求の向上に伴い、注形用エポキシ樹脂組成物においてもその硬化物に高耐熱性（分解温度）が要求されている。 Conventionally, the epoxy resin composition for casting has been used for insulating treatments such as transformers for electrical equipment and sealing of electronic parts. Such casting epoxy resin compositions are required to have stability and flame retardancy including various electrical characteristics during use. In recent years, there has been a demand for an epoxy resin composition for casting that does not contain a halogen compound or an antimony compound from the viewpoint of improving the reliability and considering the environment, and some of them have been put into practical use. In recent years, with the improvement of heat resistance requirements for electronic components, high heat resistance (decomposition temperature) is required for the cured product of the epoxy resin composition for casting.
注形用エポキシ樹脂組成物に難燃剤としてハロゲン化合物およびアンチモン化合物を用いない場合、一般に難燃剤として水酸化アルミニウムが用いられる（例えば、特許文献１参照。）。しかしながら、水酸化アルミニウムの分解温度が低いため、高温（１５０℃以上）に長時間さらされる部品については絶縁特性や強度の点に課題がある。
難燃剤として水酸化アルミニウムを用いる場合、上述したように絶縁特性や強度の点に課題があることから、これに代えて分解温度の高い水酸化マグネシウムを用いることが検討されている。 When aluminum hydroxide is used as a flame retardant, there are problems in terms of insulation characteristics and strength as described above. Therefore, it has been studied to use magnesium hydroxide having a high decomposition temperature instead.
しかしながら、水酸化マグネシウムを使用した場合、硬化物の分解温度の向上は可能となるものの、硬化前の状態である液状の状態でのチクソ性や粘度が大幅に上昇し、作業性の面に課題がある。 However, when magnesium hydroxide is used, it is possible to improve the decomposition temperature of the cured product, but the thixotropy and viscosity in the liquid state, which is the state before curing, greatly increase, and there is a problem in terms of workability. There is.
本発明は上記事情に鑑みてなされたものであって、難燃剤として分解温度の高い水酸化マグネシウムを用いることにより硬化物の耐熱性を向上させると共に、水酸化マグネシウムを用いることによる硬化前の液状の状態でのチクソ性や粘度の上昇を抑制し、作業性に優れた２液性注形用エポキシ樹脂組成物およびそれを用いた電気・電子部品装置を提供することを目的としている。 This invention is made | formed in view of the said situation, While improving the heat resistance of hardened | cured material by using magnesium hydroxide with a high decomposition temperature as a flame retardant, it is liquid before hardening by using magnesium hydroxide. It is an object of the present invention to provide a two-part casting epoxy resin composition excellent in workability by suppressing thixotropy and viscosity increase in this state, and an electric / electronic component device using the same.
本発明者らは上記目的を達成するために鋭意研究を進めた結果、後述の２液性注形用エポキシ樹脂組成物を用いることにより、上記目的を達成できることを見出し、本発明を完成したものである。 As a result of diligent research to achieve the above object, the present inventors have found that the above object can be achieved by using a two-component casting epoxy resin composition described later, and the present invention has been completed. It is.
即ち、本発明の２液性注形用エポキシ樹脂組成物は、（Ａ）ハロゲン化合物およびアンチモン化合物を含有しないエポキシ樹脂、（Ｂ）シリカ、（Ｃ）水酸化マグネシウムおよび（Ｄ）リン酸エステル系減粘剤を必須成分として含有する主剤と、（Ｅ）酸無水物硬化剤および（Ｆ）硬化促進剤を必須成分として含有する硬化剤とからなることを特徴とする。 That is, 2-component Note form epoxy resin composition of the present invention, (A) a halogen compound and containing no epoxy resin an antimony compound, (B) silica, (C) magnesium hydroxide and (D) phosphoric acid ester It is characterized by comprising a main agent containing a system thickener as an essential component, and a curing agent containing (E) an acid anhydride curing agent and (F) a curing accelerator as essential components.
本発明の２液性注形用エポキシ樹脂組成物においては、前記（Ａ）ハロゲン化合物およびアンチモン化合物を含有しないエポキシ樹脂１００重量部に対して、前記（Ｂ）シリカ３０〜１５０重量部、前記（Ｃ）水酸化マグネシウム１５０〜２５０重量部、前記（Ｄ）リン酸エステル系減粘剤０．１〜１．５重量部および前記（Ｅ）酸無水物硬化剤８０〜９０重量部であり、かつ、前記（Ｆ）硬化促進剤が前記（Ｅ）酸無水物硬化剤１００重量部に対して０．３〜５重量部であることが好ましい。 In two-part Note form epoxy resin composition of the present invention, the (A) halogen compound and antimony compound per 100 parts by weight containing no epoxy resin, (B) the silica 30 to 150 parts by weight, the (C) 150 to 250 parts by weight of magnesium hydroxide, (D) 0.1 to 1.5 parts by weight of the phosphate ester-based thinning agent, and (E) 80 to 90 parts by weight of the acid anhydride curing agent, And it is preferable that the said (F) hardening accelerator is 0.3-5 weight part with respect to 100 weight part of said (E) acid anhydride hardening | curing agents.
本発明の２液性注形用エポキシ樹脂組成物における前記（Ｄ）リン酸エステル系減粘剤は、前記（Ｄ）リン酸エステル系減粘剤は、リン酸エステル結合を有する飽和ポリエステルのコポリマーであることが好ましい。 In the two-part casting epoxy resin composition of the present invention, the (D) phosphate ester-based thickener is a copolymer of a saturated polyester having a phosphate ester bond. It is preferable that
また、本発明の電気・電子部品装置は樹脂組成物によって注形されてなる電気・電子部品装置であって、前記樹脂組成物として前記２液性注形用エポキシ樹脂組成物を用いたことを特徴とする。 The electrical / electronic component device of the present invention is an electrical / electronic component device cast by a resin composition, wherein the two-part casting epoxy resin composition is used as the resin composition. Features.
本発明によれば、主剤と硬化剤とからなる２液性注形用エポキシ樹脂組成物において、主剤に水酸化マグネシウムを添加すると共にリン酸エステル系減粘剤を添加することで、主剤における水酸化マグネシウムの添加によるチクソ性や粘度の上昇を抑制し、それにより主剤と硬化剤とを混合して得られる混合液の粘度の上昇も抑制し、作業性に優れ、かつ、硬化物の難燃性、耐熱性にも優れた２液性注形用エポキシ樹脂組成物とすることができる。 According to the present invention, in a two-part casting epoxy resin composition comprising a main agent and a curing agent, water in the main agent is added by adding magnesium hydroxide to the main agent and adding a phosphate ester-based thickener. Suppresses thixotropy and viscosity increase due to the addition of magnesium oxide, thereby suppressing the increase in viscosity of the mixture obtained by mixing the main agent and curing agent. Excellent workability and flame retardant of cured products And a heat-resistant two-component casting epoxy resin composition.
本発明の２液性注形用エポキシ樹脂組成物は、主剤と硬化剤との２液からなるものである。主剤は、（Ａ）ハロゲン化合物およびアンチモン化合物を実質的に含有しないエポキシ樹脂、（Ｂ）シリカ、（Ｃ）水酸化マグネシウムおよび（Ｄ）リン酸エステル系減粘剤を必須成分として含有するものである。また、硬化剤は、（Ｅ）酸無水物硬化剤および（Ｆ）硬化促進剤を必須成分として含有するものである。 The two-part casting epoxy resin composition of the present invention comprises two liquids, a main agent and a curing agent. The main agent contains (A) an epoxy resin substantially free of a halogen compound and an antimony compound, (B) silica, (C) magnesium hydroxide, and (D) a phosphate ester type thickener as essential components. is there. Moreover, a hardening | curing agent contains (E) acid anhydride hardening | curing agent and (F) hardening accelerator as an essential component.
まず、本発明の２液性注形用エポキシ樹脂組成物における主剤について説明する。主剤に用いられる（Ａ）エポキシ樹脂は、ハロゲン化合物およびアンチモン化合物を含有せず、１分子中に２個以上のエポキシ基を有するものであれば、分子構造、分子量などに制限されることなく、公知のエポキシ樹脂を広く使用することができる。 First, the main agent in the two-component casting epoxy resin composition of the present invention will be described. Is (A) an epoxy resin used in the base material, does not contain Ha androgenic compound and antimony compound, as long as it has two or more epoxy groups in one molecule, without limitation molecular structures, the molecular weight, etc. Well-known epoxy resins can be widely used.
（Ａ）エポキシ樹脂としては、具体的には、ビスフェノール型、ノボラック型、ビフェニル型の芳香族系、ポリカルボン酸のグリシジルエーテル、シクロヘキサン誘導体のエポキシ化によって得られる脂環属系等が挙げられる。これらのエポキシ樹脂は単独で用いてもよいし、２種類以上を混合して使用してもよい。またこれらと共に、必要に応じて液状のモノエポキシ樹脂を併用してもよい。 Specific examples of the (A) epoxy resin include bisphenol type, novolak type, biphenyl type aromatic type, glycidyl ether of polycarboxylic acid, and alicyclic group obtained by epoxidation of cyclohexane derivative. These epoxy resins may be used alone or in combination of two or more. In addition to these, a liquid monoepoxy resin may be used in combination as necessary.
主剤に用いられる（Ｂ）シリカとしては、結晶シリカや溶融シリカ等、通常充填剤として使用されるものであれば特に制限なく広く使用することができる。（Ｂ）シリカの平均粒径は、４〜２５μｍであることが好ましい。平均粒径が４μｍ未満の場合、含浸性が低下したり、主剤の粘度あるいは主剤と硬化剤とを混合したときの混合液粘度が高くなり作業性が低下することがあるため好ましくない。また、平均粒径が２５μｍを超える場合、主剤保管時や硬化時にシリカが沈降することがあるため好ましくない。 As (B) silica used for the main agent, it can be widely used without particular limitation as long as it is usually used as a filler such as crystalline silica or fused silica. (B) It is preferable that the average particle diameter of a silica is 4-25 micrometers. When the average particle size is less than 4 μm, the impregnation property is lowered, the viscosity of the main agent or the viscosity of the mixed solution when the main agent and the curing agent are mixed is increased, and workability is lowered, which is not preferable. Moreover, when an average particle diameter exceeds 25 micrometers, since a silica may precipitate at the time of main ingredient storage or hardening, it is unpreferable.
（Ｂ）シリカとしては市販品を使用することができ、例えばクリタタライトＡ−Ａ、Ａ−１、Ｃ、Ｅ−２、ＲＤ−８（いずれも株式会社龍森製、商品名）等が挙げられる。これらは単独で用いてもよいし、２種類以上を混合して使用してもよい。 (B) A commercial item can be used as silica, for example, clitalite AA, A-1, C, E-2, RD-8 (all manufactured by Tatsumori Co., Ltd., trade name) and the like. . These may be used singly or in combination of two or more.
（Ｂ）シリカは、（Ａ）エポキシ樹脂１００重量部あたり、３０〜１５０重量部の範囲で含有させることが好ましい。（Ｂ）シリカの含有量が３０重量部未満では、硬化物の強度が低下するおそれがあるため好ましくない。また、（Ｂ）シリカの含有量が１５０重量部を超えると、主剤の粘度、あるいは、主剤と硬化剤とを混合したときの混合液の粘度が高くなり作業性が低下するおそれがあるため好ましくない。 (B) Silica is preferably contained in the range of 30 to 150 parts by weight per 100 parts by weight of (A) epoxy resin. (B) If the content of silica is less than 30 parts by weight, the strength of the cured product may be lowered, which is not preferable. Further, when the content of (B) silica exceeds 150 parts by weight, the viscosity of the main agent or the viscosity of the mixed solution when the main agent and the curing agent are mixed may be increased, and workability may be reduced. Absent.
なお、必要に応じてシリカ以外の無機充填材、例えばアルミナ、タルク、炭酸カルシウム、チタンホワイト、クレー、ベンガラ、ガラス繊維および炭素繊維等を、硬化物の特性を損なわない範囲で（Ｂ）シリカと共に用いてもよい。 If necessary, inorganic fillers other than silica, such as alumina, talc, calcium carbonate, titanium white, clay, bengara, glass fiber, carbon fiber, etc., together with (B) silica, as long as the properties of the cured product are not impaired. It may be used.
主剤に用いられる（Ｃ）水酸化マグネシウムは難燃剤として使用されるものであり、水酸化アルミニウムよりも分解温度が高いため硬化物の耐熱性の向上が可能となる。（Ｃ）水酸化マグネシウムとしては、平均粒径が１〜２５μｍのものが好適に用いられる。（Ｃ）水酸化マグネシウムの平均粒径が１μｍ未満の場合、主剤の粘度あるいは主剤と硬化剤とを混合したときの混合液の粘度が高くなり、作業性が低下したり、含浸性が低下することがあるため好ましくない。また、２５μｍを超える場合、硬化物の強度が低下することがあるため好ましくない。 (C) Magnesium hydroxide used as a main agent is used as a flame retardant, and since the decomposition temperature is higher than that of aluminum hydroxide, the heat resistance of the cured product can be improved. (C) As magnesium hydroxide, a thing with an average particle diameter of 1-25 micrometers is used suitably. (C) When the average particle size of magnesium hydroxide is less than 1 μm, the viscosity of the main agent or the viscosity of the mixed solution when the main agent and the curing agent are mixed increases, and workability decreases or impregnation decreases. This is not preferable because there are cases. Moreover, when exceeding 25 micrometers, since the intensity | strength of hardened | cured material may fall, it is unpreferable.
（Ｃ）水酸化マグネシウムとしては、一般に難燃剤として使用されているものであれば天然物、合成物あるいはその表面処理品等、特に制限されることなく用いることができる。このような（Ｃ）水酸化マグネシウムとしては市販品を使用することができ、例えば水酸化マグネシウム３００、マグシーズＮ−１、Ｗ−Ｈ１０、Ｓ−１、Ｓ−３、エブソンＲＦ（神島化学工業株式会社製 商品名）等が挙げられる。これらは単独で用いてもよいし、２種類以上を混合して使用してもよい。 (C) Magnesium hydroxide can be used without particular limitation as long as it is generally used as a flame retardant, such as natural products, synthetic products or surface treated products thereof. As such (C) magnesium hydroxide, commercially available products can be used, for example, magnesium hydroxide 300, Magsees N-1, W-H10, S-1, S-3, Ebson RF (Kanjima Chemical Co., Ltd.) Company name). These may be used singly or in combination of two or more.
（Ｃ）水酸化マグネシウムは、（Ａ）エポキシ樹脂１００重量部あたり、１５０〜２５０重量部の範囲で含有させることが好ましい。（Ｃ）水酸化マグネシウムの含有量が１５０重量部未満では、硬化物の難燃性が低下するおそれがあるため好ましくない。また、（Ｃ）水酸化マグネシウムの含有量が２５０重量部を超えると、主剤の粘度、あるいは、主剤と硬化剤とを混合して得られる混合液の粘度が上昇し作業性が低下するおそれがあり、また硬化物の強度、耐湿性等が低下するおそれがあるため好ましくない。 (C) Magnesium hydroxide is preferably contained in the range of 150 to 250 parts by weight per 100 parts by weight of (A) epoxy resin. When the content of (C) magnesium hydroxide is less than 150 parts by weight, the flame retardancy of the cured product may be lowered, which is not preferable. In addition, when the content of (C) magnesium hydroxide exceeds 250 parts by weight, the viscosity of the main agent or the viscosity of a mixed liquid obtained by mixing the main agent and the curing agent may increase and workability may decrease. In addition, the strength, moisture resistance and the like of the cured product may be lowered, which is not preferable.
主剤に用いられる（Ｄ）リン酸エステル系減粘剤は、（Ｃ）水酸化マグネシウムを添加することによる主剤の粘度上昇を抑制し、これにより主剤と硬化剤とを混合したときの混合液の粘度上昇を抑制し、作業性を向上させるものである。 (D) Phosphate ester thickener used for the main agent suppresses the increase in viscosity of the main agent due to the addition of (C) magnesium hydroxide, and thus the mixture of the main agent and the curing agent is mixed. It suppresses the increase in viscosity and improves workability.
（Ｄ）リン酸エステル系減粘剤は、リン酸エステル結合を有し、粘度低下の硬化を発揮するものであればよい。具体的には、（Ｄ）リン酸エステル系減粘剤は、その分子中に樹脂と相溶性を有する部分と、（Ｂ）シリカや（Ｃ）水酸化マグネシウム等の無機充填材と吸着する部分とを有し、これら無機充填材の再凝集を防いで樹脂中に安定に存在させ、粘度低下の効果を発揮するものである。 (D) The phosphate ester type | system | group thinning agent should just have a phosphate ester bond and exhibit hardening of a viscosity fall. Specifically, the (D) phosphate ester-based thinning agent has a part that is compatible with the resin in its molecule, and a part that adsorbs to (B) an inorganic filler such as silica or (C) magnesium hydroxide. And prevents the re-aggregation of these inorganic fillers so that they are stably present in the resin and exhibit the effect of reducing the viscosity.
この（Ｄ）リン酸エステル系減粘剤としては、リン酸エステル結合を有する飽和ポリエステルのコポリマーであることが好ましい。このようなものとしては市販品を用いることもでき、例えばＢＹＫ−Ｗ９８５、Ｗ９９０、Ｗ９９５、Ｗ９９６、Ｗ９０１０（ＢＹＫ Ｃｈｅｍｉe社製 商品名）等が挙げられる。これらは単独で使用してもよいし、２種類以上を混合して使用してもよい。 The (D) phosphate ester-based thickener is preferably a saturated polyester copolymer having a phosphate ester bond. As such a thing, a commercial item can also be used, for example, BYK-W985, W990, W995, W996, W9010 (a brand name by BYK Chemie) etc. are mentioned. These may be used singly or in combination of two or more.
（Ｄ）リン酸エステル系減粘剤は（Ａ）エポキシ樹脂１００重量部に対し、０．１〜１．５重量部の範囲で含有させることが好ましい。（Ｄ）リン酸エステル系減粘剤の含有量が０．１重量部未満では、主剤、あるいは、主剤と硬化剤とを混合したときの混合液のチクソ性が強く、作業性が低下するおそれがあるため好ましくない。また、（Ｄ）リン酸エステル系減粘剤の含有量が１．５重量部を超えると、主剤、あるいは、主剤と硬化剤とを混合したときの混合液における（Ｂ）シリカ等の無機充填材の沈降が多くなり、保存安定性が低下するおそれがあるため好ましくない。 (D) It is preferable to contain a phosphate ester type | system | group thickener in 0.1-1.5 weight part with respect to 100 weight part of (A) epoxy resins. (D) When the content of the phosphate ester-based thickener is less than 0.1 parts by weight, the thixotropy of the main agent or the mixed solution when the main agent and the curing agent are mixed is strong, and the workability may be reduced. This is not preferable. In addition, when the content of (D) phosphate ester-based thinning agent exceeds 1.5 parts by weight, (B) inorganic filling such as silica in the mixed solution when the main agent or the main agent and the curing agent are mixed Since sedimentation of the material increases and storage stability may be lowered, it is not preferable.
また、本発明の２液性注形用エポキシ樹脂組成物における主剤には各成分（Ａ）〜（Ｄ）に加えて、カップリング剤、消泡剤、顔料、その他添加剤を必要に応じ、本発明の効果を阻害しない範囲で配合してもよい。 Moreover, in addition to each component (A)-(D), a coupling agent, an antifoamer, a pigment, and other additives are added to the main component in the epoxy resin composition for two-part casting of the present invention as necessary. You may mix | blend in the range which does not inhibit the effect of this invention.
次に、本発明の２液性注形用エポキシ樹脂組成物における硬化剤について説明する。硬化剤に用いられる（Ｅ）酸無水物硬化剤としては、分子中に酸無水物基を有するものであれば特に限定されるものではなく、エポキシ樹脂の硬化に一般的に使用される酸無水物硬化剤であれば広く用いることができる。 Next, the curing agent in the two-component casting epoxy resin composition of the present invention will be described. The (E) acid anhydride curing agent used for the curing agent is not particularly limited as long as it has an acid anhydride group in the molecule, and acid anhydrides generally used for curing epoxy resins. Any material curing agent can be used widely.
（Ｅ）酸無水物硬化剤としては、例えばヘキサヒドロ無水フタル酸、テトラヒドロ無水フタル酸、メチルヘキサヒドロ無水フタル酸、メチルテトラヒドロ無水フタル酸等が挙げられる。これらの酸無水物硬化剤は、単独で使用してもよいし、２種類以上を混合して使用してもよい。 Examples of (E) acid anhydride curing agents include hexahydrophthalic anhydride, tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methyltetrahydrophthalic anhydride, and the like. These acid anhydride curing agents may be used alone or in combination of two or more.
硬化剤における（Ｅ）酸無水物硬化剤は、主剤における（Ａ）エポキシ樹脂の当量に対して、９５〜１０５％の範囲となるように配合させることが好ましい。硬化剤における（Ｅ）酸無水物硬化剤の配合量が当量に対して９５％未満ではガラス転移温度が低くなる傾向にあるため好ましくない。また、硬化剤における（Ｅ）酸無水物硬化剤の配合量が当量に対して１０５％を超えると、硬化物の耐湿性等が低下するおそれがあるため好ましくない。 The (E) acid anhydride curing agent in the curing agent is preferably blended so as to be in the range of 95 to 105% with respect to the equivalent amount of the (A) epoxy resin in the main agent. If the blending amount of the (E) acid anhydride curing agent in the curing agent is less than 95% with respect to the equivalent, the glass transition temperature tends to be low, such being undesirable. Moreover, when the compounding quantity of (E) acid anhydride hardening | curing agent in a hardening | curing agent exceeds 105% with respect to an equivalent, since there exists a possibility that the moisture resistance etc. of hardened | cured material may fall, it is unpreferable.
硬化剤に用いられる（Ｆ）硬化促進剤としては、エポキシ樹脂同士、またはエポキシ樹脂と（Ｅ）酸無水物硬化剤との反応を促進する作用を有するものであればよく、そのようなものであれば特に制限されることなく用いることができる。 The (F) curing accelerator used in the curing agent may be any epoxy resin or any one having an action of promoting the reaction between the epoxy resin and the (E) acid anhydride curing agent. If there is, it can be used without any particular limitation.
（Ｆ）硬化促進剤としては、例えば２−エチル−４−エチルイミダゾール、１−シアノエチル−２−エチル−４−エチルイミダゾール、ベンジルジメチルアミン、２−（ジメチルアミノメチル）フェノール等のイミダゾール類、１，８−ジアザービシクロ（５，４，０）ウンデセン（ＤＢＵおよびそのオクチル酸塩）およびそのオクチル酸塩等の３級アミン類、トリエチルホスフィン、トリフェニルホスフィン、ジフェニルホスフィン等が挙げられる。これらは単独で使用してもよいし、２種類以上を混合して使用してもよい。 Examples of the (F) curing accelerator include imidazoles such as 2-ethyl-4-ethylimidazole, 1-cyanoethyl-2-ethyl-4-ethylimidazole, benzyldimethylamine, and 2- (dimethylaminomethyl) phenol; , 8-Diazabicyclo (5,4,0) undecene (DBU and its octylate) and tertiary amines such as octylate, triethylphosphine, triphenylphosphine, diphenylphosphine and the like. These may be used singly or in combination of two or more.
硬化剤における（Ｆ）硬化促進剤は、硬化剤における（Ｅ）酸無水物硬化剤１００重量部に対し、０．３〜５重量部の範囲となるように含有させることが好ましい。（Ｆ）硬化促進剤が０．３重量部未満であると硬化特性を十分に向上できないおそれがあるため好ましくない。また、（Ｆ）硬化促進剤が５重量部を超えると、反応が速く、ポットライフが短くなるため好ましくない。 The (F) curing accelerator in the curing agent is preferably contained so as to be in the range of 0.3 to 5 parts by weight with respect to 100 parts by weight of the (E) acid anhydride curing agent in the curing agent. (F) It is not preferable that the curing accelerator is less than 0.3 parts by weight because the curing characteristics may not be sufficiently improved. Moreover, when (F) hardening accelerator exceeds 5 weight part, since reaction is quick and a pot life becomes short, it is unpreferable.
このような本発明の２液性注形用エポキシ樹脂組成物は、以下のようにして製造することができる。まず、主剤として（Ａ）エポキシ樹脂、（Ｂ）シリカ、（Ｃ）水酸化マグネシウムおよび（Ｄ）リン酸エステル系減粘剤、必要に応じて上述したような添加剤を添加し、均一に混合して主剤を得る。また、（Ｅ）酸無水物硬化剤および（Ｆ）硬化促進剤を添加し、均一に混合して硬化剤を得る。 Such a two-component casting epoxy resin composition of the present invention can be produced as follows. First, add (A) epoxy resin, (B) silica, (C) magnesium hydroxide, and (D) phosphate ester thickener as necessary, and add additives as described above, if necessary, and mix uniformly. To obtain the main agent. Also, (E) an acid anhydride curing agent and (F) a curing accelerator are added and mixed uniformly to obtain a curing agent.
このような主剤および硬化剤からなる２液性注形用エポキシ樹脂組成物は、電気・電子部品装置の製造に好適に用いられる。電気・電子部品装置の製造は、例えば主剤と硬化剤とを混合して混合液とした後、これを電気部品や電子部品が収容されたケース内に注入し、必要に応じて７０〜８０℃、２〜４時間、その後１００〜１２０℃、２〜４時間の加熱を行い硬化させることにより行う。 Such a two-component casting epoxy resin composition comprising a main agent and a curing agent is suitably used for the production of electrical / electronic component devices. For example, the electrical / electronic component device is manufactured by mixing a main agent and a curing agent to form a mixed solution, and then injecting the mixed solution into a case in which the electrical component or the electronic component is accommodated. 2 to 4 hours, and then heating at 100 to 120 ° C. for 2 to 4 hours for curing.
本発明の２液性注形用エポキシ樹脂組成物を用いて製造される電気・電子部品装置としては、例えばコイルやトランスをはじめとする電気・電子部品装置が挙げられる。このような電気・電子部品装置の製造に本発明の２液性注形用エポキシ樹脂組成物を用いれば、耐熱性に優れた電気・電子部品装置の製造が可能となる。また、本発明の２液性注形用エポキシ樹脂組成物は粘度が低く、具体的には主剤、あるいは、主剤と硬化剤とを混合して得られる混合液の粘度が低く抑えられているため作業性に優れ、電気・電子部品装置を容易に製造することができる。 Examples of the electric / electronic component device manufactured using the two-component casting epoxy resin composition of the present invention include an electric / electronic component device including a coil and a transformer. If the two-component casting epoxy resin composition of the present invention is used for the production of such an electric / electronic component device, it is possible to produce an electric / electronic component device having excellent heat resistance. In addition, the two-part casting epoxy resin composition of the present invention has a low viscosity, and specifically, the viscosity of a mixed liquid obtained by mixing a main agent or a main agent and a curing agent is kept low. It is excellent in workability and can easily produce an electric / electronic component device.
次に、本発明を実施例によりさらに詳細に説明する。本発明はこれらの実施例によって限定されるものではない。 Next, the present invention will be described in more detail with reference to examples. The present invention is not limited by these examples.
（実施例１〜４、比較例１〜２）
ハロゲン化合物およびアンチモン化合物を実質的に含有しないエポキシ樹脂、シリカ、水酸化マグネシウムおよびリン酸エステル系減粘剤、その他添加剤を配合、混合して主剤とし、またこれとは別に酸無水物硬化剤および硬化促進剤を配合、混合して硬化剤とし、実施例１〜４の２液性注形用エポキシ樹脂組成物を得た。
(Examples 1-4, Comparative Examples 1-2)
An epoxy resin substantially free of halogen compounds and antimony compounds, silica, magnesium hydroxide, phosphate ester-based thickeners, and other additives are blended and mixed into the main agent. Separately, acid anhydride curing agents And the hardening accelerator was mix | blended and mixed and it was set as the hardening | curing agent, and the epoxy resin composition for two-component casting of Examples 1-4 was obtained.
また、比較例１〜２として、リン酸エステル系減粘剤を含有しない主剤および硬化剤を作製し２液性注形用エポキシ樹脂組成物を得た。実施例１〜４および比較例１、２の２液性注形用エポキシ樹脂組成物における主剤および硬化剤の成分およびその含有量は表１に示す通りとした。なお、表１における含有量は重量部で示した。また、各成分の詳細は以下に示す通りである。 Moreover, as Comparative Examples 1-2, the main ingredient and hardening | curing agent which do not contain a phosphate ester type | system | group thinning agent were produced, and the epoxy resin composition for two-component casting was obtained. Components of the main agent and the curing agent and their contents in the two-part casting epoxy resin compositions of Examples 1 to 4 and Comparative Examples 1 and 2 were as shown in Table 1. In addition, content in Table 1 was shown by the weight part. Moreover, the detail of each component is as showing below.
（主剤）
ハロゲン化合物およびアンチモン化合物を実質的に含有しないエポキシ樹脂：ビスフェノールＡ型エポキシ樹脂 ＥＰ４１００Ｅ（旭電化工業株式会社製 商品名）、ビスフェノールＦ型エポキシ樹脂 エピコート８０７（油化シェルエポキシ株式会社製 商品名）、モノエポキサイド カージュラＥ１０（油化シェルエポキシ株式会社製 商品名）。
シリカ：クリスタライトＡ−１（株式会社龍森製 商品名、平均粒径１１μｍ）。
水酸化マグネシウム：マグシーズＳ−１、マグシーズＳ−３（いずれも神島化学工業株式会社製 商品名、平均粒径４．０μｍ、１．０μｍ）。
水酸化アルミニウム：Ｈ４２Ｉ、Ｈ３１Ｉ（いずれも昭和電工株式会社製 商品名、平均粒径１μｍ、１５μｍ）。
リン酸エステル系減粘剤：ＢＹＫ９０１０（ＢＹＫ Ｃｈｅｍｉｅ社製 商品名）。
消泡剤：ＴＳＡ７２０（東芝シリコーン株式会社製 商品名）。
シランカップリング剤：ＴＳＬ８３５０（東芝シリコーン株式会社製 商品名）。
(Main agent)
Epoxy resin substantially free of halogen compound and antimony compound: bisphenol A type epoxy resin EP4100E (trade name, manufactured by Asahi Denka Kogyo Co., Ltd.), bisphenol F type epoxy resin Epicoat 807 (product name, manufactured by Yuka Shell Epoxy Co., Ltd.), Mono epoxide side Cardura E10 (trade name, manufactured by Yuka Shell Epoxy Co., Ltd.).
Silica: Crystallite A-1 (trade name, manufactured by Tatsumori Co., Ltd., average particle size 11 μm).
Magnesium hydroxide: Magseeds S-1 and Magseeds S-3 (both trade names, average particle size 4.0 μm, 1.0 μm, manufactured by Kamishima Chemical Co., Ltd.).
Aluminum hydroxide: H42I, H31I (both trade names, average particle size 1 μm, 15 μm, manufactured by Showa Denko KK).
Phosphate ester-based thickener: BYK9010 (trade name, manufactured by BYK Chemie).
Antifoaming agent: TSA720 (trade name, manufactured by Toshiba Silicone Co., Ltd.).
Silane coupling agent: TSL8350 (trade name, manufactured by Toshiba Silicone Co., Ltd.).
（硬化剤）
酸無水物硬化剤：ＱＨ２００（日本ゼオン株式会社製 商品名）。
硬化促進剤：２Ｅ４ＭＺ−ＣＮ（四国化成工業株式会社製 商品名）。
(Curing agent)
Acid anhydride curing agent: QH200 (trade name, manufactured by Nippon Zeon Co., Ltd.).
Curing accelerator: 2E4MZ-CN (trade name, manufactured by Shikoku Kasei Kogyo Co., Ltd.).
次に、実施例１〜４、比較例１、２の２液性注形用エポキシ樹脂組成物について、主剤の粘度、主剤の沈降性を測定した。また、主剤と硬化剤とを混合して得た混合液の粘度を測定した。結果を表２に示す。なお、粘度の測定はＢ型粘度計（主剤粘度および比較例１の混合液粘度：Ｎｏ．４ロータ、０．６ｒｐｍ。その他の混合液粘度：Ｎｏ．３ロータ、１２ｒｐｍ。）を用いて２５℃で測定した。沈降性の測定は１００℃で２時間静置したときの沈降物の有無を測定することにより行った。表１中、○を付けたものは沈降物がほとんどなかったものを表し、×を付けたものは沈降物が多かったものを表す。 Next, the viscosity of the main agent and the sedimentation property of the main agent were measured for the two-component casting epoxy resin compositions of Examples 1 to 4 and Comparative Examples 1 and 2. Moreover, the viscosity of the liquid mixture obtained by mixing a main ingredient and a hardening | curing agent was measured. The results are shown in Table 2. The viscosity was measured at 25 ° C. using a B-type viscometer (main agent viscosity and mixed solution viscosity of Comparative Example 1: No. 4 rotor, 0.6 rpm. Other mixed solution viscosity: No. 3 rotor, 12 rpm). Measured with The sedimentation was measured by measuring the presence or absence of sediment when left at 100 ° C. for 2 hours. In Table 1, those marked with ◯ represent those with little sediment, and those marked with x represent those with much sediment.
さらに、各実施例１〜４、比較例１、２の２液性注形用エポキシ樹脂組成物について、主剤と硬化剤とを混合、硬化して得られる硬化物の難燃性、ガラス転移点および５％分解温度を測定した。結果を表２に示す。なお、難燃性の評価は厚さ６．４ｍｍの硬化物を試料として、ＵＬ９４試験に基づいて行った。また、ガラス転移点の測定はＴＭＡ法に基づいて行った。 Furthermore, about the epoxy resin composition for two-component casting of each of Examples 1 to 4 and Comparative Examples 1 and 2, flame retardancy of a cured product obtained by mixing and curing the main agent and a curing agent, glass transition point And 5% decomposition temperature was measured. The results are shown in Table 2. The evaluation of flame retardancy was performed based on the UL94 test using a cured product having a thickness of 6.4 mm as a sample. The glass transition point was measured based on the TMA method.
表２から明らかなように、実施例１〜４の２液性注形用エポキシ樹脂組成物においては、ハロゲン化合物およびアンチモン化合物を含まないものの水酸化マグネシウムを含有しているためいずれもその硬化物は難燃性に優れることが認められた。また、実施例１〜４の２液性注形用エポキシ樹脂組成物においては、リン酸エステル系減粘剤を含有しているため、主剤の粘度および主剤と硬化剤とを混合したときの混合液の粘度が低く抑えられており、作業性に優れていることが認められた。 As is apparent from Table 2, the two-part casting epoxy resin compositions of Examples 1 to 4 do not contain a halogen compound and an antimony compound, but contain magnesium hydroxide, both of which are cured products. Was found to be excellent in flame retardancy. In addition, in the two-part casting epoxy resin composition of Examples 1 to 4, since it contains a phosphate ester-based thickener, the viscosity of the main agent and mixing when the main agent and the curing agent are mixed It was confirmed that the viscosity of the liquid was kept low and the workability was excellent.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2004030449A JP4540997B2 (en) | 2004-02-06 | 2004-02-06 | Two-component casting epoxy resin composition and electrical / electronic component equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2004030449A JP4540997B2 (en) | 2004-02-06 | 2004-02-06 | Two-component casting epoxy resin composition and electrical / electronic component equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2005220256A JP2005220256A (en) | 2005-08-18 |
| JP4540997B2 true JP4540997B2 (en) | 2010-09-08 |
Family
ID=34996146
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2004030449A Expired - Fee Related JP4540997B2 (en) | 2004-02-06 | 2004-02-06 | Two-component casting epoxy resin composition and electrical / electronic component equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4540997B2 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5255762B2 (en) * | 2005-12-29 | 2013-08-07 | アキレス株式会社 | Acrylic resin composition and sheet-like molded body using the same |
| JP6051557B2 (en) * | 2012-03-26 | 2016-12-27 | 日立化成株式会社 | Epoxy resin liquid sealing material for underfill and electronic component device |
| JP2014028931A (en) * | 2012-06-26 | 2014-02-13 | Sanyo Chem Ind Ltd | Grout material composition for reinforcing steel bar joint |
| CN112143171A (en) * | 2019-07-15 | 2020-12-29 | 上海闰龙电子材料有限公司 | Formula and preparation method of high-flame-retardancy epoxy resin potting material |
| JP7616071B2 (en) | 2019-12-16 | 2025-01-17 | 株式会社レゾナック | Thermosetting resin composition |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1060096A (en) * | 1996-08-20 | 1998-03-03 | Toshiba Chem Corp | Flame-retardant epoxy resin composition |
| JPH1171503A (en) * | 1997-08-29 | 1999-03-16 | Hitachi Chem Co Ltd | Epoxy resin composition and insulation treatment of electric instrument using the same |
| JP2000053875A (en) * | 1998-06-02 | 2000-02-22 | Nitto Denko Corp | Semiconductor sealing resin composition, semiconductor device using the same and method for manufacturing semiconductor device |
| JP2001316590A (en) * | 2000-05-02 | 2001-11-16 | Kyowa Chem Ind Co Ltd | Material for sealing electronic parts, resin composition for sealing electronic parts and moldings thereof |
| JP2004224827A (en) * | 2003-01-20 | 2004-08-12 | Murata Mfg Co Ltd | Resin composition for casting high voltage part |
-
2004
- 2004-02-06 JP JP2004030449A patent/JP4540997B2/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1060096A (en) * | 1996-08-20 | 1998-03-03 | Toshiba Chem Corp | Flame-retardant epoxy resin composition |
| JPH1171503A (en) * | 1997-08-29 | 1999-03-16 | Hitachi Chem Co Ltd | Epoxy resin composition and insulation treatment of electric instrument using the same |
| JP2000053875A (en) * | 1998-06-02 | 2000-02-22 | Nitto Denko Corp | Semiconductor sealing resin composition, semiconductor device using the same and method for manufacturing semiconductor device |
| JP2001316590A (en) * | 2000-05-02 | 2001-11-16 | Kyowa Chem Ind Co Ltd | Material for sealing electronic parts, resin composition for sealing electronic parts and moldings thereof |
| JP2004224827A (en) * | 2003-01-20 | 2004-08-12 | Murata Mfg Co Ltd | Resin composition for casting high voltage part |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2005220256A (en) | 2005-08-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5642917B2 (en) | Epoxy resin composition for impregnating mold coil and mold coil apparatus | |
| JP6329043B2 (en) | Epoxy resin composition for two-part casting and electronic component | |
| JP5314379B2 (en) | Epoxy resin composition for mold coil impregnation casting, mold coil device and method for manufacturing mold coil device | |
| JP2000510497A (en) | Epoxy resin casting composition | |
| JP4540997B2 (en) | Two-component casting epoxy resin composition and electrical / electronic component equipment | |
| JP2009114222A (en) | Epoxy resin composition for casting and electric/electronic component device | |
| JP6357089B2 (en) | Two-component casting epoxy resin composition, method for producing the epoxy resin composition, and coil component | |
| JP3872038B2 (en) | Casting epoxy resin composition, curing method thereof, and electric / electronic component device | |
| JP6348401B2 (en) | Epoxy resin composition for impregnation casting, coil component and method for producing the same | |
| JP6804992B2 (en) | Epoxy resin composition for coil impregnation, manufacturing method of coil products, and ignition coil | |
| JPH1060096A (en) | Flame-retardant epoxy resin composition | |
| JP2008038017A (en) | Flexible epoxy resin composition for casting and electric/electronic part device | |
| JP2007277469A (en) | Casting epoxy resin composition and electric/electronic part apparatus | |
| JP2005048100A (en) | Epoxy resin composition for casting and electrical/electronic component apparatus | |
| JP2003147047A (en) | Epoxy resin composition for casting and electric or electronic part device | |
| JP2002155193A (en) | Epoxy resin composition and electrical/electronic component device | |
| JPH1087964A (en) | Epoxy resin composition for cast molding | |
| JP2016134562A (en) | Coil impregnating resin composition and coil component | |
| JPH10292090A (en) | Epoxy resin composition for casting | |
| JP2006117806A (en) | Epoxy resin composition for casting and electronic component device | |
| JP2005048101A (en) | Epoxy resin composition for casting and electrical/electronic component apparatus | |
| JPH1060229A (en) | Flame-retardant epoxy resin composition | |
| JP3949436B2 (en) | Casting epoxy resin composition and electrical / electronic component equipment | |
| JPH0940747A (en) | Castable epoxy resin composition | |
| JP2005023220A (en) | Flame-retardant epoxy resin composition, electric or electronic component insulated by using the same, and method for producing the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20061127 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20090827 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20091222 |
|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20100217 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20100622 |
|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20100623 |
|
| R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130702 Year of fee payment: 3 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130702 Year of fee payment: 3 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20140702 Year of fee payment: 4 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20140702 Year of fee payment: 4 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313111 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| LAPS | Cancellation because of no payment of annual fees |